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Abstract: With ultrasonic irradiation as assistance, highly dispersed MoO3 nanospheres were synthesized using silane coupling agent 3-mercaptopropyltrimethoxysilane HS-(CH2)3Si(OCH3)3 (MPTS) as figuration agent. The results of X-ray powder diffractometer (XRD) showed that the precursor was hexagonal molybdenum oxide hydrate (MoO3 0.55H2O). It was converted into orthorhombic MoO3 after annealed at 400°C for 2h. Transmission electron microscopy (TEM) showed that MoO3 ·0.55H2O and MoO3 nanoparticles were spherical with particle-size distribution of ca. 30–80nm and 25–75nm, respectively. Results indicated that MPTS and ultrasonic irradiation played important role in formation of highly dispersed MoO3 nanospheres. X-ray photoelectron spectroscopy (XPS) was also adopted to confirm the growth mechanism. The possible cause of formation was based on dispersion function of ultrasonic irradiation and figuration of MPTS. [Copyright &y& Elsevier]